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Potassium Hydroxide → HCID 22267595、化合物

HRID 2298016
ノート
印刷プレビュー

反応式

HRID 2298016 の反応式
[C:1]1([N:7]2[N:11]=[C:10]([C:12]([O:14][CH3:15])=[O:13])[C:9]([C:16]([O:18]C)=[O:17])=[N:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[OH-].[K+]>CO>[CH3:15][O:14][C:12]([C:10]1[C:9]([C:16]([OH:18])=[O:17])=[N:8][N:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[N:11]=1)=[O:13]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 14344840dimethyl 2-phenyl-2H-1,2,3-triazole-4,5-dicarboxylate

生成物 1

HCID 22267595HCID 22267595、化合物収率 85%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

反応条件

温度
23 °C

実験手順

A solution of dimethyl 2-phenyl-2H-1,2,3-triazole-4,5-dicarboxylate (0.522 g, 2.00 mmol) in methanol (40 mL) at 23° C. was treated with a solution of KOH (0.236 g, 4.20 mmol) in methanol (5 mL). The resulting solution was stirred at 23° C. for 17 h and partitioned between NaHCO3 (sat. aq. sol.) and ether. The aqueous layer was washed with ether and acidified carefully to pH 1 with HCl (conc.). The resulting mixture, was extracted with EtOAc. The organic extract was washed with brine, dried over MgSO4 and concentrated in vacuo. The residue was purified by radial chromatography (2 mm plate, CH2Cl2-methanol-acetic acid 90:10:1) to afford 0.42 g (85%) of 5-methoxycarbonyl-2-phenyl-2H-1,2,3-triazole-4carboxylic acid.

後処理

  1. custompartitioned between NaHCO3 (sat. aq. sol.) and ether
  2. washThe aqueous layer was washed with ether
  3. extractionThe resulting mixture, was extracted with EtOAc
  4. extractionThe organic extract
  5. washwas washed with brine
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated in vacuo
  8. customThe residue was purified by radial chromatography (2 mm plate, CH2Cl2-methanol-acetic acid 90:10:1)

出典と根拠

ORDレコード
ord-fdce6ff289cb4506a59c108329a540c6
出典データセット
uspto-grants-2002_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06492401B1

反応ノート

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